HRID1297029

反应详情

EQUATION

反应方程式

HRID 1297029 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.5 ml of a solution of 610 mg (1.84 mmol) of (3,3-diphenylpropane-1-yl)4-chloroacetoacetate in THF was added dropwise to a suspension of 158 mg (3.95 mmol) of sodium hydride (60% oily) in 5 ml of THF at 0° C., and they were stirred at room temperature for 20 minutes. An alkoxide solution previously prepared by adding 397 mg (3.09 mmol) of 2-cyclohexylethanol to 5 ml of a solution of 134 mg (3.36 mmol) of sodium hydride (60% oily) in THF was added to the obtained mixture at 0° C., and they were stirred at room temperature for 3 nights. THF was evaporated under reduced pressure. Water was added to the residue. The obtained mixture was washed with ethyl acetate. The aqueous layer was acidified with 2 N hydrochloric acid. After the extraction with ethyl acetate followed by drying over sodium sulfate, ethyl acetate was evaporated under reduced pressure to obtain the title compound.

WORKUP

后处理

  1. additionwas added to the obtained mixture at 0° C.
  2. stirringthey were stirred at room temperature for 3 nights
  3. customTHF was evaporated under reduced pressure
  4. additionWater was added to the residue
  5. washThe obtained mixture was washed with ethyl acetate
  6. extractionAfter the extraction with ethyl acetate
  7. dry with materialby drying over sodium sulfate, ethyl acetate
  8. customwas evaporated under reduced pressure